p-Chlorothiophenol → 2-(4-Chlorophenylthio)-1-(4-methylphenyl)ethanone

HRID 2187634

反応式

HRID 2187634 の反応式
[CH3:1][C:2]1[CH:11]=[CH:10][C:5]([C:6](=[O:9])[CH2:7]Br)=[CH:4][CH:3]=1.[Cl:12][C:13]1[CH:18]=[CH:17][C:16]([SH:19])=[CH:15][CH:14]=1.C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[Cl:12][C:13]1[CH:18]=[CH:17][C:16]([S:19][CH2:7][C:6]([C:5]2[CH:10]=[CH:11][C:2]([CH3:1])=[CH:3][CH:4]=2)=[O:9])=[CH:15][CH:14]=1

参加物

5

反応物 3

HCID 7815p-ChlorothiophenolHCID 11430Potassium CarbonateHCID 692722-Bromo-4'-methylacetophenone

生成物 1

HCID 27451012-(4-Chlorophenylthio)-1-(4-methylphenyl)ethanone収率 82.3%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
80 °C

実験手順

A mixture of 10.0 g (47 mmol) 4-methylphenacyl bromide, 6.8 g (47 mmol) 4-chlorothiophenol, and 6.5 g (47 mmol) anhydrous potassium carbonate in 100 ml dry DMF was stirred for 3 h at 80° C. It was filtered and the filtrate was concentrated under reduced pressure. The concentrate was stirred in water, and the resulting solid was filtered off, washed with water, and recrystallized from ethanol to give 10.7 g (82%) of the crude title compound.

後処理

  1. filtrationIt was filtered
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. stirringThe concentrate was stirred in water
  4. filtrationthe resulting solid was filtered off
  5. washwashed with water
  6. customrecrystallized from ethanol

出典と根拠

ORDレコード
ord-44f50bf5ebd84717b40adb93417d9ac3
出典データセット
uspto-grants-2002_06
特許番号
US06410562B1

関連ノート

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